Supercritical Carbon Dioxide Extraction Research Articles

Parametric and kinetic study of supercritical carbon dioxide extraction on sinensetin from Orthosiphon stamineus Benth. leaves

ABSTRACT Sinensetin is a rare polymethoxyflavone that possesses strong anti-angiogenesis activity that can be obtained from Orthosiphon stamineus (O. stamineus) leaves. In this study, supercritical carbon dioxide (SC-CO2) extraction was used to improve sinensetin recovery from O. stamineus leaves. The effect of mean particle size (400–550, 550–650 and 650–750 µm), modifier ratio (0, 5 and 10%, v/v), flow rate (3, 4 and 5 mL/min), temperature (40, 60 and 80 °C) and pressure (10, 20 and 30 MPa) on the concentration of sinensetin and determine its extraction rate were investigated. Two models, viz. Patricelli and Peleg were used to evaluate the kinetic behavior of sinensetin in the SC-CO2 system. Results showed that the highest concentration of sinensetin was successfully extracted at 550–650 µm, 10% (v/v), 5 mL/min, 80 °C and 10 MPa. Also, the kinetic profile of sinensetin was well correlated with Patricelli and Peleg models with a low percentage average absolute relative deviation (AARD%) and a high coefficient of determination (R2) of <6.37% and >0.974, respectively. Thus, the fastest extraction rate of sinensetin was obtained at 9.039 × 10−3 mg/g min−1 using the Patricelli model and 8.694 × 10−3 mg/g min−1 using the Peleg model at 40 °C and 30 MPa.

Supercritical Carbon Dioxide Extraction, Antioxidant Activity, and Fatty Acid Composition of Bran Oil from Rice Varieties Cultivated in Portugal

Bran of different rice cultivars produced in Portugal were used to study supercritical carbon dioxide extraction conditions of rice bran oil (RBO) and evaluate and compare antioxidant activity and fatty acid composition of the different rice bran varieties. The effect of plant loading (10–20 g), CO2 flow rate (0.5–1.5 L/min), pressure (20–60 MPa), and temperature (40–80 °C) was studied. The amount of oil extracted ranged from 11.72%, for Ariete cultivar, to 15.60%, for Sirio cultivar. The main fatty acids components obtained were palmitic (13.37%–16.32%), oleic (44.60%–52.56%), and linoleic (29.90%–38.51%). Excellent parameters of the susceptibility to oxidation of the oils were obtained and compare. RBO of Ariete and Gladio varieties presented superior DPPH and ABTS radical scavenging activities, whereas, Minima, Ellebi, and Sirio varieties had the lowest scavenging activities. Moreover, the oil obtained towards the final stages of extraction presented increased antioxidant activity.

Carbon dioxide supercritical fluid extracts from yarrow and rose hip herbal dust as valuable source of aromatic and lipophilic compounds

The present study was designed to demonstrate the potential of supercritical extracts from Achillea millefolium and Rosa canina herbal dust, and their mixtures, as a source of valuable aromatic and lipophilic compounds. The supercritical carbon dioxide extraction (SFE-CO2) was performed at the pressures from 10-30 MPa, providing the total extraction yields (EY) in the range from 0.12 to 10.57%, being the highest when pure R. canina herbal dust was extracted using SFE-CO2 at 30 MPa for 5 h. Chemical profiles of SFE-CO2 extracts were determined by GC-MS and GC-FID. Oxygenated monoterpenes and sesquiterpene hydrocarbons were among the most abundant compounds in the extracts produced from A. millefolium and mixtures with a higher share of A. millefolium herbal dust. In the same mixtures, at the pressure of 10 MPa, a cosolvent effect was observed, which provided enhanced extraction of eucalyptol. The major tocol in A. millefolium and R. canina mixtures was α-tocopherol (589.49 mg/L). By investigating the influence of extraction pressure, it has been determined that higher compound recoveries could be obtained at lower pressures. The results clearly demonstrate that SFE-CO2 extracts of the A. millefolium and R. canina and their herbal dust mixtures are a promising source of valuable compounds to be used in pharmaceutical formulations.

Brief characteristics of oxidative stability, fatty acids and metal content in selected berry seed extracts obtained by the SFE technique and used as potential source of nutrients

Berry seeds are rich source of high quality oil containing valuable compounds such as polyunsaturated fatty acids and therefore, have been gaining increasing significance as potential source of nutrients for food, cosmetic or pharmaceutical industry. Supercritical carbon dioxide extraction of seeds was performed, for which oxidative stability analyzes and determinations of fatty acids, selected microelements and toxic metals were carried out. An attempt was made to evaluate unclassified scCO2 oil extracts from berry seeds, taking into account the lack of legislative documents specifying the required contents of metals and biologically active ingredients. The obtained extracts are products with the consistency of liquid oil. The total fatty acid content range from 59% to 98%, with unsaturated fatty acids predominating and very good n-3/n-6 fatty acids ratio. The analyzed samples were taken systematically from one extraction sequence also determining the acid and the peroxide values in subsequent fractions.

Recovery of Moringa oleifera Oil from Seed Cake by Supercritical Carbon Dioxide Extraction

Recovery of Moringa oleifera Oil from Seed Cake by Supercritical Carbon Dioxide Extraction

Advances in Supercritical Carbon Dioxide Extraction of Bioactive Substances from Different Parts of Ginkgo biloba L.

Ginkgo biloba L. has always been a popular area of research due to its various active ingredients and pharmacological effects. Ginkgo biloba is rich in ginkgo flavonoids, ginkgolides, and ginkgolic acid, with anti-inflammation, antioxidation, neuroprotection, anti-platelet agglutination, hypolipidemic effect, anti-cancer, and anti-radiation properties. There are many methods to extract and separate the active components of ginkgo. Among them, supercritical carbon dioxide fluid extraction (SFE-CO2) is known for its green, clean, and environment-friendly properties. In this paper, the pharmacological activities, the active components, and structures of different parts of ginkgo, the extraction methods of its effective ingredients, and the application of the SFE-CO2 method for the extraction and separation of active ingredients in Ginkgo biloba from leaves, seeds, pollen, and roots were reviewed, in order to make best use of ginkgo resources, and provide support and references for the development of SFE-CO2 of active components from Ginkgo biloba.

Supercritical Carbon Dioxide Extraction of Hevea Brasiliensis Seeds: Influence of Particle Size on to Oil Seed Recovery and its Kinetic

The aim of this study is to investigate the effect of particle sizes on yield, diffusivity, mass transfer and morphological characterization on extraction rate of rubber seed oil recovery by supercritical carbon dioxide (ScCO2). Pressure 30 MPa, temperature 60 oC and average particle size 500 µm gives the maximum oil recovery (34.71%), diffusivity coefficient (5.13 E-12 m2/s) and extraction rate (0.6 mg/sec). The morphological characterization of extracted rubber seeds was done on the basis of scanning electron microscopy which was parallel with the results of the effect of particle size. The results obtained from gas chromatography-mass spectrometry showed that the rubber seeds oil contained significant essential fatty acids and certain chemical constituents which are very valuable.

Extraction of Rice Bran Oil from Rice Bran by Supercritical Carbon Dioxide

Extraction of Rice Bran Oil from Rice Bran by Supercritical Carbon Dioxide

The Modulation of PCSK9 and LDLR by Supercritical CO2 Extracts of Mentha longifolia and Isolated Piperitone Oxide, an In Vitro Study.

In the present study the ability of supercritical carbon dioxide (SCO2) extracts of M. longifolia L. leaves to modulate low-density lipoprotein receptor (LDLR) and proprotein convertase subtilisin/kexin type 9 (PCSK9) expression was evaluated in cultured human hepatoma cell lines Huh7 and HepG2. Two SCO2 extracts, one oil (ML-SCO2) and a semisolid (MW-SCO2), were subjected to detailed chemical characterization by mono- and bidimensional nuclear magnetic resonance (1D, 2D-NMR), gas chromatography coupled with mass spectrometry (GC-MS) and liquid chromatography coupled with mass spectrometry (LC-MS). Chemical analysis revealed significant amounts of fatty acids, phytosterols and terpenoids. ML-SCO2 was able to induce LDLR expression at a dose of 60 µg/mL in HuH7 and HepG2 cell lines. Furthermore, ML-SCO2 reduced PCSK9 secretion in a concentration-dependent manner in both cell lines. Piperitone oxide, the most abundant compound of the volatile constituent of ML-SCO2 (27% w/w), was isolated and tested for the same targets, showing a very effective reduction of PCSK9 expression. The overall results revealed the opportunity to obtain a new nutraceutical ingredient with a high amount of phytosterols and terpenoids using the SCO2 extraction of M. longifolia L., a very well-known botanical species used as food. Furthermore, for the first time we report the high activity of piperitone oxide in the reduction of PCSK9 expression.

Procyanidin and proanthocyanidin extraction from Arachis hypogaea skins by using supercritical carbon dioxide: Optimization and modeling

The goal of this study is to recover high procyanidins and proanthocyanidins as promising compounds from Arachis hypogaea skin using supercritical carbon dioxide (ScCO2). Solubility models determined the solubility of procyanidins and proanthocyanidins in ScCO2 and ethanol as a modifier. The parameters of this study were pressure (10 to 30 MPa), temperature (313 to 343 K), and flow rate of ethanol (0.075 to 0.225 ml/min). Response surface methodology (RSM) revealed that the optimum conditions were at 20.39 MPa, 333.23 K, and 0.17 ml/min with 2,325.23- and 409.95-µg/g procyanidins and proanthocyanidins, respectively. In the modeling part, the Chrastil model gave the best correlation to the flavonoids' solubility with 3.01% of average absolute relative deviation (AARD). The application of RSM and modeling were successful in obtaining a high amount of procyanidins and proanthocyanidins. Practical applications Peanut skin as agriculture by-products contains highly valuable compounds such as procyanidins and proanthocyanidins. However, toxic and conventional solvent has usually been used to recover procyanidins and proanthocyanidins. To overcome this drawback, supercritical carbon dioxide (ScCO2) extraction is applied to extract the valuable compounds from peanut skin. Semiempirical model has been used in this study to determine the solubility behavior to enhance the solubility of procyanidin and proanthocyanidin contents. The results show that an endothermic reaction took place to improve the solubility.

Recovery of bioactive compounds from walnut (Juglans regia L.) green husk by supercritical carbon dioxide extraction

SummaryIn this work, the use of supercritical carbon dioxide, a nontoxic solvent, was proposed to extract bioactive compounds from Juglans regia L. green husk and was compared to other traditional techniques based on solvents such as ethanol, methanol and water. Supercritical CO2 was combined with ethanol as an organic modifier at a rate of 20% of the total flow to achieve greater extraction of polar compounds. The extracts were characterised in terms of extraction yields, antioxidant activity, total polyphenol content, phenolic acids, juglone, volatile organic compounds and antifungal activity. The results showed that the extracts obtained with supercritical CO2 were rich in polyphenols (10750 mg GAE/100 g) and juglone (1192 mg/100 g) and exerted high antioxidant activity and antifungal activity compared with the tested fungi. Walnut green husk is not just a food industry waste but also an important economic source of bioactive compounds that could be used for food active packaging.

Enhancement of Lipid Extraction from Soya Bean by Addition of Dimethyl Ether as Entrainer into Supercritical Carbon Dioxide.

Soya beans contain a variety of lipids, and it is important to selectively separate neutral lipids from other lipids. Supercritical carbon dioxide extraction has been used as an alternative to the selective separation of neutral lipids from soya beans, usually using non-polar hexane. However, supercritical carbon dioxide extraction has a high operating pressure of over 40 MPa. On the other hand, liquefied dimethyl ether extraction, which has attracted attention in recent years, requires an operating pressure of only 0.5 MPa, but there is concern about the possibility of an explosion during operation because it is a flammable liquefied gas. Therefore, this study aims to reduce the operating pressure by using a non-flammable solvent, supercritical carbon dioxide extraction mixed with liquefied dimethyl ether as an entrainer. The extraction rate and the amount of neutral lipids extracted increased with increasing amounts of added liquefied dimethyl ether. In the mixed solvent, the amount of neutral lipids extracted was higher at an operating pressure of 20 MPa than in pure supercritical carbon dioxide extraction at 40 MPa. The mixing of liquefied dimethyl ether with supercritical carbon dioxide allowed an improvement in the extraction of neutral lipids while remaining non-flammable.

Development and Optimization of Supercritical Fluid Extraction Setup Leading to Quantification of 11 Cannabinoids Derived from Medicinal Cannabis.

Simple SummaryThis study describes the design and development of setup for the extraction of cannabis strain 1 (Cannabidiol dominant) using supercritical carbon dioxide. For this purpose, two different supercritical fluid extraction instruments were used. The extraction conditions were maintained at 37 °C and 250 bar. Different carbon dioxide inlet and outlet positions were experimented to obtain the maximum yield. A separating chamber was also designed to reduce the throttling effect and dry ice formation during the depressurization process. After developing the supercritical fluid extraction setup, ultra-high performance liquid chromatography coupled with a diode array detection quantification method for 11 cannabinoids was developed.In this study, the optimal setup of supercritical fluid extraction (SFE) was designed and developed, leading to the quantitation of 11 distinct cannabinoids (cannabidivann (CBDV), tetrahydrocannabivann (THCV), cannabidiol (CBD), cannabigerol (CBG) cannabidiolic acid (CBDA), cannabigerolic acid (CBGA), cannabinol (CBN), delta 9-tetrahydrocannabinol (Δ9-THC), delta 8-tetrahydrocannabinol (Δ8-THC), cannabichomere (CBC) and delta 9-tetrahydrocannabinol acid (THCA-A)) extracted from the flowers of medicinal cannabis (sp. Sativa). Supercritical carbon dioxide (scCO2) extraction was performed at 37 °C, a pressure of 250 bar with the maximum theoretical density of CO2 (893.7 kg/m3), which generated the highest yield of cannabinoids from the flower-derived extract. Additionally, a cold separator (separating chamber) was used and positioned immediately after the sample containing chamber to maximize the yield. It was also found that successive washing of the extract with fresh scCO2 further increased yields. Ultra-high performance liquid chromatography coupled with DAD (uHPLC-DAD) was used to develop a method for the quantification of 11 cannabinoids. The C18 stationary phase was used in conjunction with a two solvent system gradient program resulting in the acquisition of the well-resolved chromatogram over a timespan of 32 min. The accuracy and precision of isolated cannabinoids across inter-and intra-day periods were within acceptable limits (<±15%). The assay was also fully validated and deemed sensitive from linearity, LOQ, and LOD perspective. The findings of this body of work are expected to facilitate improved conditions for the optimal extraction of select cannabinoids using scCO2, which holds promise in the development of well-characterized medicinal cannabis formulations. As to our best knowledge, this is the first study to report the uHPLC quantification method for the analysis of 11 cannabinoids from scCO2 extract in a single run with more than 1 min peak separation.

Screening of Functional Compounds in Supercritical Carbon Dioxide Extracts from Perennial Herbaceous Crops

The bio-based economy concept requires using biomass not only for energy production but also for bioactive compound extraction, application or biotransformation. This study analyzed the possibility of obtaining bioactive compounds from biomass before its transformation into biofuel. This involved an analysis of the total content of polyphenols (TPC), flavonoids (TFC), and spectral analysis using Fourier transform infrared spectroscopy (QATR- FTIR) as well as analysis of the antioxidant activity of extracts from selected perennial herbaceous crops cultivated on marginal lands in Poland. The extracts were obtained by supercritical carbon dioxide extraction (scCO2) or scCO2 with water as a cosolvent (scCO2/H2O) from biomass of the following plants: Helianthus salicifolius, Silphium perfoliatum, Helianthus tuberosus, Miscanthus × giganteus, Miscanthus sacchariflorus, Miscanthus sinensis and Spartina pectinata. The biomass was harvested twice during the growing period (June and October) and once after the end of the growing period (February). For most of the analyzed extracts obtained from biomass at the growing stage using scCO2 or scCO2/H2O, a higher TPC was noted than for samples of semi-wood or straw biomass obtained after the end of the growing period. Higher contents of polyphenolic compounds were recorded in extracts obtained using scCO2/H2O. A positive correlation between TPC and antioxidant activity was noted for the analyzed substrates. Flavonoid contents varied in the analyzed samples, and higher contents were generally obtained in scCO2 extracts from biomass harvested at the beginning of the growing period. A high diversity of extract compositions was confirmed by spectral analysis. The presented data can be used at the initial stage of planning a biorefinery.

Innovative recycling of organic binders from electric vehicle lithium-ion batteries by supercritical carbon dioxide extraction

The growing demand for energy storage devices due to the skyrocketing production/consumption of portable electrical and electronic equipment as well as electric vehicles has promoted battery technologies, resulting in the piling of a large number of waste lithium-ion batteries (LIBs). Organic binders wrapped on electrode particles are usually the main reason that causes the difficulty of liberation and extraction of electrode materials. Pyrolysis or incineration is the general approach to separate the organic binder, leading to fluorinated exhaust gas emissions. In this study, the supercritical carbon dioxide (SC CO2) combined with a cosolvent dimethyl sulfoxide was innovatively adapted to enable the extraction of organic binders from spent LIBs to facilitate the liberation of the cathode material from aluminum foil. Pure polyvinylidene fluoride was preferentially used to study the SC CO2 dissolution mechanism. The results indicate that 98.5 wt% polyvinylidene fluoride (PVDF) dissolves in SC CO2 dimethyl sulfoxide system under the optimum conditions; 70°C process temperature, 80 bar pressure, and 13 min duration. After removing PVDF, the recovered sample was characterized by Fourier Transform Infrared Spectrometer (FTIR) and thermogravimetric analyzer (TGA) to observe its possible re-utilization. It is clear that the surficial chemical groups and content remained the same after treatment. SC CO2 processing effectively liberates the active cathode material from the aluminum substrate due to removal of the binder. The suggested innovative approach is promising as an alternative pretreatment method due to its high efficiency, relatively low energy consumption, and environmentally friendly features.

Role of virgin coconut oil (VCO) as co-extractant for obtaining xanthones from mangosteen (Garcinia mangostana) pericarp with supercritical carbon dioxide extraction

Virgin coconut oil (VCO) was used as co-extractant with supercritical carbon dioxide (scCO2) extraction for obtaining xanthones from mangosteen pericarp (MP) without organic co-solvents. In each experiment, 120 g of dried MP that had median particle sizes of 0.85 mm was used. Extraction of MP with 40% VCO co-extractant using scCO2 (1.08 kg/h) for 420 min at 430 bar and 70 °C gave α-mangostin (32.2 mg/g), γ-mangostin (7.2 mg/g), xanthones (28.2 mg/g) in extract and an extraction yield of 31%. The role of VCO is that it promotes dissolution of xanthones and mass transfer into the scCO2 phase as elucidated with the Pardo-Castaño model. The Lentz equation was generalized in terms of (P, T, %VCO, ρCO2) to correlate all extraction curve data to within 7.4% and to estimate extraction yield crossover regions. Xanthones can be separated from mangosteen pericarp with VCO and scCO2 extraction without organic co-solvents.

Identification of the fatty acids profiles in supercritical CO2 fluid and Soxhlet extraction of Samara oil from different cultivars of Elaeagnus mollis Diels seeds

Nutritional values in five cultivars of Elaeagnus mollis Diels seeds were evaluated. The profiles of fatty acids in samara oil (SO1 to SO5), extracted from five cultivars of Elaeagnus mollis Diels seeds were identified by GC–MS. Two extraction technologies, supercritical fluid carbon dioxide (SF-CO2) and Soxhlet extraction were also compared. A higher oil yield was obtained through Soxhlet extraction against SF-CO2 technology. SF-CO2-Extracted SO obtained higher unsaturated fatty acid (USFA) content, while Soxhlet-Extracted SO had higher saturated fatty acid (SFA) content. The ratio of USFA to SFA was 9:1. Linoleic acid, oleic acid, and palmitic acid were the most abundant fatty acids identified in SO. The content ratio of linoleic acid to α-Linolenic acid in SO4 was close to the proportions in breast milk (6:1). SO1 and SO4 could be used as potential sources to develop functional food products. SF-CO2 technology was a better option for SO extraction regarding preservation of bioactive compounds.

Comparative Studies of Selected Criteria Enabling Optimization of the Extraction of Polar Biologically Active Compounds from Alfalfa with Supercritical Carbon Dioxide

The aim of this research was to provide crucial and useful data about the selection of the optimization criteria of supercritical carbon dioxide extraction of alfalfa at a quarter-technical plant. The correlation between more general output, including total phenolics and flavonoids content, and a more specified composition of polar constituents was extensively studied. In all alfalfa extracts, polar bioactive constituents were analyzed by both spectrometric (general output) and chromatographic (detailed output) analyses. Eight specific phenolic acids and nine flavonoids were determined. The most dominant were salicylic acid (221.41 µg g−1), ferulic acid (119.73 µg g−1), quercetin (2.23 µg g−1), and apigenin (2.60 µg g−1). For all seventeen analyzed compounds, response surface methodology and analysis of variance were used to provide the optimal conditions of supercritical fluid extraction for each individual constituent. The obtained data have shown that eight of those compounds have a similar range of optimal process parameters, being significantly analogous for optimization based on total flavonoid content.

Process optimization for the supercritical carbondioxide extraction of lycopene from ripe grapefruit (Citrus paradisi) endocarp

In this study, an underutilized citrus family fruit named grapefruit was explored for the extraction of lycopene using supercritical carbon dioxide (CO2) extraction technique. An experimental design was developed using response surface methodology to investigate the effect of supercritical carbon dioxide (CO2) operating parameter viz., pressure, temperature, CO2 flow rate, and extraction time on the extraction yield of lycopene yield from grapefruit. A total of 30 sets of experiments were conducted with six central points. The statistical model indicated that extraction pressure and extraction time individually, and their interaction, significantly affected the lycopene yield. The central composite design showed that the polynomial regression models developed were in agreement with the experimental results, with R2 of 0.9885. The optimum conditions for extraction of lycopene from grapefruit were 305 bar pressure, 35 g/min CO2 flow rate, 135 min of extraction time, and 70 °C temperature.

Clove (Syzygium aromaticum) spices: a review on their bioactivities, current use, and potential application in dairy products

Clove is a common spice used as a flavorant and natural preservative in food industries due to its rich phenolic constituents like eugenol and eugenol acetate etc. These phenolic constituents possess enormous antioxidant activities, anti-glycation, antinociceptive and antimicrobial properties which enhanced the bioactivities of clove spices. Several in vitro and in vivo assays have been conducted to ascertain the potentials of clove spices as well as its cytotoxicity. Due to its beneficial effects, clove spices have been applied for use in agriculture as insecticides, anesthesia, antioxidants etc. In general, methods used for processing of herbs and spices including clove spices are drying, solvent extraction, microwave assisted extraction, supercritical carbondioxide extraction, ultrasound assisted extraction and microencapsulation. All of these were reviewed and presented in this article. Previous findings on application of spices and herbs in dairy products were eye-opener which suggested that clove spices could be incorporated into dairy products. Consequently, it will help to promote clove spices as potential nutraceutical and food additive in different foods particularly in dairy products.